机构地区:[1]贵州省农业科学院植物保护研究所,贵阳550006
出 处:《农药》2022年第5期350-357,369,共9页Agrochemicals
基 金:黔农科院青年基金[2017]16号。
摘 要:[目的]为探明敌草隆和环嗪酮在甘蔗上使用后的残留特性和安全性,建立了QuEChERS-超高效液相色谱-串联质谱法测定甘蔗、甘蔗植株及土壤中敌草隆与环嗪酮残留的分析方法。[方法]样品经1%乙酸-乙腈(V:V)提取,甘蔗以PSA净化,甘蔗植株以PSA+GCB净化,土壤以C_(18)净化,UHPLC-MS/MS检测,外标法定量。在贵州和海南进行了敌草隆和环嗪酮在甘蔗和甘蔗田土壤的田间消解动态及最终残留试验。[结果]0.0005~2.0 mg/L范围内,敌草隆和环嗪酮在3种基质中质量浓度与对应的峰面积间线性关系良好(R^(2)>0.99);在0.001、0.5、2.0 mg/kg添加水平下,敌草隆的回收率为80%~115%,RSD为3.21%~13.17%;环嗪酮的回收率为68%~109%,RSD为0.68%~8.06%;2种农药的方法定量限LOQ和检出限LOD均为0.001 mg/kg。敌草隆和环嗪酮在甘蔗和土壤中的降解动力学模型比较发现曲棍球模型HS动力学拟合效果更好,HS模型预测下敌草隆甘蔗上半衰期(DT_(50))为5.65、0.94 d,在土壤中为5.07、3.07 d;环嗪酮在甘蔗植株中半衰期为2.00、0.29 d,在土壤中为1.95、2.65 d。敌草隆在甘蔗上的最终残留为<LOQ~0.009 mg/kg,环嗪酮为<LOQ~0.004 mg/kg,土壤中敌草隆最终残留量为0.004~0.091 mg/kg,环嗪酮为<LOQ~0.002 mg/kg。甘蔗中敌草隆与环嗪酮在不同性别的各类人群中的长期膳食摄入风险评价均为可接受风险。[结论]甘蔗上使用60%环嗪酮·敌草隆水分散粒剂,施药时间在甘蔗4~6叶期施药1次,有效剂量不超过2430 g a.i./hm2,不会造成甘蔗中敌草隆与环嗪酮残留超标和引起长期膳食摄入风险。[Aims]In order to investigate the residual characteristic and safety of diuron and hexazinone in sugarcane,QuEChERS-ultra-performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)method was developed for the determination of diuron and hexazinone in sugarcane,sugarcane plants and soil.[Methods]Samples were extracted by 1%acetic acid-acetonitrile(by vol),cleaned up by PSA,PSA+GCB and C_(18) for sugarcane,sugarcane plants and soil,respectively,detected by UHPLC-MS/MS,and quantified by external standard method.The dissipation dynamics and final residue trials of diuron and hexazinone in sugarcane and sugarcane fields were investigated by this method carried out in Guizhou and Hainan Provinces.[Results]The calibration curve with good linearity was obtained in the concentration range of 0.0005 to 2.0 mg/L(R^(2)>0.99).At 0.001,0.5 and 2.0 mg/kg spiking levels,the average recoveries of diuron in the three matrices was 80-115%with the RSD≤13.17%,and hexazinone was 68-109%with RSD of 0.68-8.06%.The limit of quantitative(LOQ)and limit of detection(LOD)of the two pesticides in these matrices were 0.001 mg/kg.The residues of diuron and hexazinone in sugarcane and soil decreased with time.Comparison of degradation kinetic models showed that the measured data could fitting effect of Hockey stick kinetic model(HS)was better.The half-lives(DT_(50))of diuron in sugarcane plant predicted is 5.65 and 0.94 d,and in soil it is 5.07 and 3.07 d.Half-lives of hexazinone are 2.00 and 0.29 d in sugarcane plant,and 1.95 and 2.65 d in soil.The respective final residues of diuron and hexazinone in sugarcane were<0.001-0.009 and<0.001-0.004 mg/kg,in soil were 0.004-0.091 and<0.001-0.002 mg/kg.Long-term dietary intake risk assessment of diuron and hexazinone in sugarcane is acceptable.[Conclusions]The application of hexazinone and diuron 60%water dispersible granules in sugarcane is carried out once at the 4 to 6th leaf stage,and the effective dose is not more than 2430 g a.i./ha,which will not cause the residues of diuron and
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...
正在载入数据...